CN105158517A - Method of in-situ observation of nanometer material growth in liquid environment - Google Patents
Method of in-situ observation of nanometer material growth in liquid environment Download PDFInfo
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- CN105158517A CN105158517A CN201510553618.5A CN201510553618A CN105158517A CN 105158517 A CN105158517 A CN 105158517A CN 201510553618 A CN201510553618 A CN 201510553618A CN 105158517 A CN105158517 A CN 105158517A
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Abstract
The invention discloses a method of in-situ observation of nanometer material growth in a liquid environment. The method is characterized in that a liquid cavity for in-situ observation of a nanometer material is formed by butted bonding of metal support grids covered with carbon films; a reaction solution drops on one side, with the carbon film, of the bottom metal support grid by a liquid transfer gun, and one side, covered with the carbon film, of another metal support grid is placed downwardly by a pair of tweezers and covers the bottom metal support grid with the solution; after the rest of solution is evaporated, the metal support grids are bonded together based on the bonding forces and van der waals' forces of the carbon films, thereby forming an enclosed cavity; and the reaction solution is sealed in the cavity. According to the invention, the provided method has advantages of low cost, simple operation, and high resolution and the like; observation of the nanometer material in a liquid environment can be carried out conveniently and rapidly; and development of the in-situ observation technology of the nanometer material can be effectively promoted.
Description
Technical field
The present invention relates to a kind of method adopting New body cavity to carry out home position observation nano material growth under liquid environment, belong to the fluid chamber preparation method in original position electron microscopy observation technology.
Background technology
Nano material refers to the material having at least a yardstick in nanometer scale, has the performance that small-size effect, bulk effect, quantum effect etc. are different from bulk material.The physical characteristics of these uniquenesses that nano material has each technical field such as medical equipment, electronic equipment, coating is biological, medical that makes it be widely used in.But due to the naked eyes invisibility of nano material and the low enlargement factor of optical microscope and resolution, the observation of nano material must by the Electron Microscopy taking electron beam as imaging source.
The essential states of direct observation sample has been the important goal of electron microscope since invention, and traditional electron microscopy need make sample observe under high vacuum environment, requires that sample must be anhydrous and without volatile reagent.But a lot of sample (especially biomaterial) state is under vacuo greatly different with state in a solvent, dry run during sample preparation often causes the structure of sample, and great changes will take place, thus be difficult to the native mode observing sample, the course of reaction in in-situ observation solution can not realize especially.2003, the people such as the Williamson of University of Virginia proposed a kind of method preparing fluid chamber, observed the deposit of Cu on Au surface under liquid environment, had started the beginning of in-situ observation nano material under liquid environment since then.In more than ten years in the past, observe the technology of nano material obtain and develop fast under liquid environment, being prepared in the process of this technical development of fluid chamber plays a part pole and closes important.The technology of current preparation fluid chamber can be divided into two large classes, and the first kind adopts two panels to the transparent silicon nitride film of electron beam by liquid-packing, and the thickness of silicon nitride film and the thickness of liquid level cause being difficult to realize high-resolution imaging and observation.Preparing silicon nitride fluid chamber needs through series of steps such as spin coating, deposition, etching, bonding and encapsulation, complex process, and be difficult to the quality ensureing silicon nitride film, the thinnest silicon nitride film can prepared at present, cannot the character of the nano material of accurate surveying smaller szie further at about 13nm.Equations of The Second Kind is single-layer graphene fluid chamber, because single-layer graphene only has the thickness of a carbon atom, so can ensure the high resolving power of atom magnitude.But Graphene is subject to electron beam irradiation appearance breakage under high voltage electron microscope environment, is difficult to the long-time observation ensureing nano material, the breakage of graphene film simultaneously can cause fluid leakage, and then produces adverse influence to Electronic Speculum state.Simultaneously when preparing Graphene fluid chamber, need first on Copper Foil, to grow single-layer graphene, then Graphene being transferred to the metal being coated with amorphous carbon film carries on the net, again the metal of two panels load Graphene is carried net to sticky, make two panels metal carry online graphene film to inhale together because adhesion etc. acts on, the last metal removing top again carries net, and the method complex steps and success ratio are difficult to ensure.Two kinds that more than introduce use fluid chamber technology of preparing widely all to have preparation is complicated, length consuming time and the success ratio shortcoming being difficult to ignore such as low, seriously constrain the fast development of in-situ observation nano material technology under liquid environment, thus seek the fluid chamber technology of preparing that a kind of preparation method is simple, low for equipment requirements, success ratio is high, the cycle is short and there is important practical value and meaning.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the invention provides the method for home position observation nano material growth under a kind of liquid environment, be a kind of fluid chamber technology of preparing that can be used for nano material characteristic in Electron Microscopy situ observation liquid environment, this technology can realize quick, the low cost preparation of fluid chamber.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
A method for home position observation nano material growth under liquid environment, the method comprises the steps:
(1) underlying metal of a slice load carbon film being carried net level is placed on filter paper or microslide, and underlying metal carries one of net load carbon film and faces up; The order number that underlying metal carries net is 10 ~ 1000 orders;
(2) liquid-transfering gun is utilized to drop on carbon film by the reaction solution of 2 ~ 5 μ L; Reaction solution has difference because of its wellability state that underlying metal carries net surface that do not coexist, but need ensure that reaction solution carries at underlying metal as far as possible and be evenly distributed on the net;
(3) top-level metallic of another sheet load carbon film is carried net level to cover and drip the underlying metal of solution of responding and carry on the net, top-level metallic carries one of net load carbon film and faces down, and double layer of metal carries net and reaction solution forms sandwich structure; Top-level metallic carries that net and underlying metal carry the specification of net, material is identical, and top-level metallic carries net and covers underlying metal when carrying online, ensures that each grid, netting twine are just right; Specification, the material of two-layer carbon film are identical, and thickness is 5 ~ 15nm;
(4) ensure that sandwich structure is static, treat that surplus liquid evaporates, two-layer carbon film is bonded together due to the effect such as adhesion and Van der Waals force, forms airtight chamber, is sealed in chamber by reaction solution and forms fluid chamber; Surplus liquid evaporation time concrete visual response solution composition and determine;
(5) fluid chamber is placed on specimen holder, under moving to transmission electron microscope, carries out the in-situ observation of the nano material growth under liquid environment.
A kind of preferred version, carries the magnificent film in the side of being provided with between net and the carbon film of load at underlying metal, and to carry between net and the carbon film of load the also magnificent film in the side of being provided with at top-level metallic, just magnificent film can ensure the sealing of chamber further.
Another kind of preferred version, carry between net and the carbon film of load at underlying metal and be provided with porous organic film, carry between net and the carbon film of load at top-level metallic and be also provided with porous organic film, porous organic film can ensure the sealing of chamber further.
Preferably, described top-level metallic carries net and underlying metal to carry net is copper mesh, nickel screen or golden net.
In implementation process of the present invention, transmission electron microscope can be used and the equipment such as the electron microscope sample bar that matches with it.
Beneficial effect: the method for home position observation nano material growth under liquid environment provided by the invention, prepare a kind of novel fluid chamber, compared with existing fluid chamber technology of preparing, the present invention utilizes the strong adhesion between carbon film and Van der Waals force to be sealed by liquid between two panels carbon film, form airtight liquid chamber, the nano material character under in-situ observation liquid environment can be ensured; This method, without the need to buying other special equipment, only needs the metal of the magnificent film in the two panels side of being coated with and carbon film to carry net, and liquid-transfering gun, tweezers and a transmission electron microscope are with low cost; Simultaneously the present invention is without the need to the technological process of complexity, consuming time short, is the method for a kind of quick, economy home position observation nano material growth under liquid environment easily.
Accompanying drawing explanation
Fig. 1 is the schematic diagram obtaining fluid chamber according to the present invention;
Fig. 2 is the image of Au nano particle under transmission electron microscope utilizing fluid chamber of the present invention to close.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further described.
Embodiment 1
A slice load side China's film and the copper grid of carbon film are placed on microslide, face up containing that of film.Utilize liquid-transfering gun to drop on carbon film by the solution containing nano material of 3 μ L, adopt liquid-transfering gun tip that liquid is distributed at carbon film surface uniform.That of another magnificent film in sheet copper grid load side of having and carbon film faced down with tweezers, covering to drip has the base copper of solution to carry on the net.Keep this accurate fluid chamber system quiescence.Treat that redundant solution evaporates, the carbon film on copper grid surface sticks together due to the acting force such as adhesion and Van der Waals force, forms airtight chamber, reaction solution is enclosed in the inside, and the magnificent film in side can ensure the sealing of liquid further.Treat that fluid chamber is prepared complete, place it on specimen holder, under moving to electron microscope, carry out the in-situ observation of the nano ZnO under liquid environment.
Embodiment 2
The copper grid of supported porous for a slice organic film and ultrathin carbon films is placed on microslide, faces up containing that of film.Utilize liquid-transfering gun to drop on carbon film by the solution that 3 μ L contain nano material, adopt liquid-transfering gun tip that liquid is distributed at carbon film surface uniform.That another sheet copper grid load being had porous organic film and a ultrathin carbon films with tweezers faces down, and covering to drip has the base copper of solution to carry on the net.Keep this accurate fluid chamber system quiescence.Treat that redundant solution evaporates, the carbon film on copper grid surface sticks together due to the acting force such as adhesion and Van der Waals force, forms airtight chamber, reaction solution is enclosed in the inside.Treat that fluid chamber is prepared complete, place it on specimen holder, under moving to electron microscope, carry out the in-situ observation of the nano ZnO under liquid environment.
Embodiment 3
The copper grid of a slice load carbon film is placed on microslide, faces up containing that of film.Utilize liquid-transfering gun to drop on carbon film by the solution that 3 μ L contain nano material, adopt liquid-transfering gun tip that liquid is distributed at carbon film surface uniform.That of another sheet copper grid load carbon film faced down with tweezers, covering to drip has the base copper of solution to carry on the net.Keep this accurate fluid chamber system quiescence.Treat that redundant solution evaporates, the carbon film on copper grid surface sticks together due to the acting force such as adhesion and Van der Waals force, forms airtight chamber, reaction solution is enclosed in the inside.Treat that fluid chamber is prepared complete, place it on specimen holder, under moving to electron microscope, carry out the in-situ observation of the nano ZnO under liquid environment.
Embodiment 4
The load side's China's film adopted according to embodiment 1 and the copper grid of carbon film carry out the encapsulation of fluid chamber, in the airtight chamber formed size after the bonding of two panels carbon film is entered in the water-soluble fluid-tight of the Au nano particle of 10 ~ 20nm.Packaged fluid chamber is placed on specimen holder, under moving to transmission electron microscope, carries out the in-situ observation of the nano ZnO under liquid environment.Image display under transmission electron microscope, aqueous solution flows under the irradiation of electron beam, drives gold nano grain to move together.As shown in Figure 2.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a method for home position observation nano material growth under liquid environment, is characterized in that: the method comprises the steps:
(1) underlying metal of a slice load carbon film being carried net level is placed on filter paper or microslide, and underlying metal carries one of net load carbon film and faces up; The order number that underlying metal carries net is 10 ~ 1000 orders;
(2) liquid-transfering gun is utilized to drop on carbon film by the reaction solution of 2 ~ 5 μ L;
(3) top-level metallic of another sheet load carbon film is carried net level to cover and drip the underlying metal of solution of responding and carry on the net, top-level metallic carries one of net load carbon film and faces down, and double layer of metal carries net and reaction solution forms sandwich structure; Top-level metallic carries that net and underlying metal carry the specification of net, material is identical, and top-level metallic carries net and covers underlying metal when carrying online, ensures that each grid, netting twine are just right; Specification, the material of two-layer carbon film are identical, and thickness is 5 ~ 15nm;
(4) ensure that sandwich structure is static, treat that surplus liquid evaporates, two-layer carbon film is bonded together, and forms airtight chamber, is sealed in chamber by reaction solution and forms fluid chamber;
(5) fluid chamber is placed on specimen holder, under moving to transmission electron microscope, carries out the in-situ observation of the nano material growth under liquid environment.
2. the method for home position observation nano material growth under liquid environment according to claim 1, is characterized in that: carry the magnificent film in the side of being provided with between net and the carbon film of load at underlying metal, to carry between net and the carbon film of load the also magnificent film in the side of being provided with at top-level metallic.
3. the method for home position observation nano material growth under liquid environment according to claim 1, it is characterized in that: carry between net and the carbon film of load at underlying metal and be provided with porous organic film, carry between net and the carbon film of load at top-level metallic and be also provided with porous organic film.
4. the method for home position observation nano material growth under liquid environment according to claim 1, is characterized in that: described top-level metallic carries net and underlying metal, and to carry net be copper mesh, nickel screen or golden net.
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Cited By (6)
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| CN106990265A (en) * | 2017-04-02 | 2017-07-28 | 浙江大学 | A kind of carbon-based transmission electron microscope sample contained network and preparation method thereof |
| CN108226572A (en) * | 2017-12-29 | 2018-06-29 | 国联汽车动力电池研究院有限责任公司 | A kind of atomic force microscope sample scaling method |
| CN109164121A (en) * | 2018-08-01 | 2019-01-08 | 华东师范大学 | The preparation method of self assembly in-situ liquid chamber for transmission electron microscope characterization |
| CN110632105A (en) * | 2019-09-17 | 2019-12-31 | 东南大学 | Liquid sample cavity for transmission electron microscope characterization and preparation method thereof |
| CN111999149A (en) * | 2020-09-08 | 2020-11-27 | 厦门大学 | Carbon film liquid pool and preparation method thereof |
| CN114878612A (en) * | 2022-05-10 | 2022-08-09 | 北京理工大学 | Sample preparation method for solving carbon pollution phenomenon of nanocrystals in TEM (transmission electron microscope) representation |
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Cited By (8)
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| CN106990265A (en) * | 2017-04-02 | 2017-07-28 | 浙江大学 | A kind of carbon-based transmission electron microscope sample contained network and preparation method thereof |
| CN108226572A (en) * | 2017-12-29 | 2018-06-29 | 国联汽车动力电池研究院有限责任公司 | A kind of atomic force microscope sample scaling method |
| CN109164121A (en) * | 2018-08-01 | 2019-01-08 | 华东师范大学 | The preparation method of self assembly in-situ liquid chamber for transmission electron microscope characterization |
| CN109164121B (en) * | 2018-08-01 | 2020-10-16 | 华东师范大学 | Preparation method of self-assembly in-situ liquid cavity for transmission electron microscope characterization |
| CN110632105A (en) * | 2019-09-17 | 2019-12-31 | 东南大学 | Liquid sample cavity for transmission electron microscope characterization and preparation method thereof |
| CN111999149A (en) * | 2020-09-08 | 2020-11-27 | 厦门大学 | Carbon film liquid pool and preparation method thereof |
| CN114878612A (en) * | 2022-05-10 | 2022-08-09 | 北京理工大学 | Sample preparation method for solving carbon pollution phenomenon of nanocrystals in TEM (transmission electron microscope) representation |
| CN114878612B (en) * | 2022-05-10 | 2024-01-30 | 北京理工大学 | Sample preparation method for solving carbon pollution phenomenon of nanocrystals in TEM (transmission electron microscope) characterization |
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Application publication date: 20151216 |